JP2015506821A5 - - Google Patents
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- JP2015506821A5 JP2015506821A5 JP2014546274A JP2014546274A JP2015506821A5 JP 2015506821 A5 JP2015506821 A5 JP 2015506821A5 JP 2014546274 A JP2014546274 A JP 2014546274A JP 2014546274 A JP2014546274 A JP 2014546274A JP 2015506821 A5 JP2015506821 A5 JP 2015506821A5
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- 239000003054 catalyst Substances 0.000 claims description 29
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 25
- 239000010457 zeolite Substances 0.000 claims description 22
- 239000002808 molecular sieve Substances 0.000 claims description 21
- 150000002910 rare earth metals Chemical class 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- -1 rare earth compound Chemical class 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N AI2O3 Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N Adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- YGSDEFSMJLZEOE-UHFFFAOYSA-N Salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 4
- 239000004005 microsphere Substances 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- PZZYQPZGQPZBDN-UHFFFAOYSA-N Aluminium silicate Chemical compound O=[Al]O[Si](=O)O[Al]=O PZZYQPZGQPZBDN-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- ILRRQNADMUWWFW-UHFFFAOYSA-K Aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N Boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- KARVSHNNUWMXFO-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane;hydrate Chemical compound O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O KARVSHNNUWMXFO-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 229910052621 halloysite Inorganic materials 0.000 claims description 2
- 235000011167 hydrochloric acid Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 229960004889 salicylic acid Drugs 0.000 claims description 2
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 239000011975 tartaric acid Substances 0.000 claims description 2
- 235000002906 tartaric acid Nutrition 0.000 claims description 2
- 229960001367 tartaric acid Drugs 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 17
- 239000006185 dispersion Substances 0.000 claims 13
- 238000000034 method Methods 0.000 claims 6
- 238000001354 calcination Methods 0.000 claims 5
- 239000002270 dispersing agent Substances 0.000 claims 5
- 239000002002 slurry Substances 0.000 claims 5
- 229910052809 inorganic oxide Inorganic materials 0.000 claims 4
- 235000012970 cakes Nutrition 0.000 claims 3
- 239000004927 clay Substances 0.000 claims 3
- 229910052570 clay Inorganic materials 0.000 claims 3
- 238000010304 firing Methods 0.000 claims 3
- 239000000295 fuel oil Substances 0.000 claims 3
- 238000002360 preparation method Methods 0.000 claims 3
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims 3
- 229910052708 sodium Inorganic materials 0.000 claims 3
- 239000011734 sodium Substances 0.000 claims 3
- 238000005406 washing Methods 0.000 claims 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N Benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims 2
- 229910052684 Cerium Inorganic materials 0.000 claims 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims 2
- 150000003863 ammonium salts Chemical class 0.000 claims 2
- 238000004523 catalytic cracking Methods 0.000 claims 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims 2
- 229910052746 lanthanum Inorganic materials 0.000 claims 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N precursor Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims 2
- 229910017119 AlPO Inorganic materials 0.000 claims 1
- 239000005711 Benzoic acid Substances 0.000 claims 1
- 239000004113 Sepiolite Substances 0.000 claims 1
- 240000008700 Sesbania cannabina Species 0.000 claims 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N Silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims 1
- 235000010233 benzoic acid Nutrition 0.000 claims 1
- 239000002131 composite material Substances 0.000 claims 1
- TUKQLEWOUPCTOS-UHFFFAOYSA-N dimagnesium;dioxido(oxo)silane;hydroxy-oxido-oxosilane;hydrate Chemical compound O.[Mg+2].[Mg+2].O[Si]([O-])=O.O[Si]([O-])=O.[O-][Si]([O-])=O TUKQLEWOUPCTOS-UHFFFAOYSA-N 0.000 claims 1
- 229910001562 pearlite Inorganic materials 0.000 claims 1
- 229910052624 sepiolite Inorganic materials 0.000 claims 1
- 235000019355 sepiolite Nutrition 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- DVARTQFDIMZBAA-UHFFFAOYSA-O Ammonium nitrate Chemical compound [NH4+].[O-][N+]([O-])=O DVARTQFDIMZBAA-UHFFFAOYSA-O 0.000 description 1
- 241000219782 Sesbania Species 0.000 description 1
- NTOVTTDJIUNDJQ-UHFFFAOYSA-N [NH4+].[NH4+].[O-]S([O-])(=O)=O.OC(=O)C(O)=O Chemical compound [NH4+].[NH4+].[O-]S([O-])(=O)=O.OC(=O)C(O)=O NTOVTTDJIUNDJQ-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- QDHHCQZDFGDHMP-UHFFFAOYSA-N monochloramine Chemical compound ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Description
本発明に記載する触媒組成におけるほかのモレキュラーシーブは、Y型ゼオライト、Lゼオライト、ZSM-5ゼオライト、βゼオライト、リン酸アルミニウムゼオライト、Ωゼオライトから選ばれる1種又は1種以上ものもであり、好ましいのはY型ゼオライト、ZSM-5ゼオライト、βゼオライト、或は上記のゼオライトの通常の物理又は化学変性されたものであり、HY、USY、REY、REHY、REUSY、H-ZSM-5、Hβを含む。 Other molecular sieves in the catalyst composition described in the present invention are Y type zeolite, L zeolite, ZSM-5 zeolite, β zeolite, aluminum phosphate zeolite, and one or more types selected from Ω zeolite, Preferred is Y-type zeolite, ZSM-5 zeolite, β- zeolite, or the usual physical or chemical modification of the above-mentioned zeolite, HY, USY, REY, REHY, REUSY, H-ZSM-5, H Contains β .
実施例に用いられる原料の仕様について
1.NaYモレキュラーシーブ:NaY-1(ケイバン比4.8、結晶化度92%)、NaY-2(ケイバン比4.1、結晶化度83%)、蘭州石化社触媒工場製。
2.超安定1交換1焼成モレキュラーシーブサンプル:結晶化度60%、酸化ナトリウム4.3m%、蘭州石化社触媒工場製。
3.希土類溶液:塩化希土類(酸化希土類 277.5g/l)、硝酸希土類(酸化希土類 252g/l)、いずれも工業製品であり、蘭州石化社触媒工場から得られるもの。
4.セスバニア粉、ホウ酸、尿素、エタノール、ポリアクリルアミド、シュウ酸、アジピン酸、酢酸、ギ酸、塩酸、硝酸、クエン酸、サリチル酸、酒石酸、デンプンはいずれも化学用ものであり;塩化アンモニウム、硝酸アンモニウム、硫酸アンモニウム、シュウ酸アンモニウムはいずれも工業製品である。
5.擬ベーマイト(熱灼減量36.2%)、カオリン(熱灼減量16.4%)、ハロイサイト(熱灼減量21.4%)、モンモリロナイト(熱灼減量15.8%)、パーライト(熱灼減量17.6%)は、固体であり;アルミニウムゾルは酸化アルミニウムを23.0重量%含み;シリコンゾルはシリカを24.5重量%含み、いずれも工業合格品である。
6.REY、REHY、USY、REUSYモレキュラーシーブは、いずれも合格工業品であり、蘭州石化社触媒工場製;βゼオライトは、工業合格品、撫順石化社製;H-ZSM-5は、工業合格品、上海復旦大学製。
About specifications of raw materials used in Examples 1. NaY molecular sieve: NaY-1 (Kayban ratio 4.8, crystallinity 92%), NaY-2 (Kayban ratio 4.1, crystallinity 83%), manufactured by Lanzhou Petrochemical Co., Ltd. Catalyst Factory.
2. Ultra-stable 1 exchange 1 calcined molecular sieve sample: 60% crystallinity, 4.3m% sodium oxide, manufactured by Lanzhou Petrochemical Company.
3. Rare earth solution: rare earth chloride (rare earth oxide 277.5g / l), rare earth nitrate (rare earth oxide) 252g / l), both industrial products, obtained from Lanzhou Petrochemical's catalyst factory.
4). Sesbania powder, boric acid, urea, ethanol, polyacrylamide, oxalic acid, adipic acid, acetic acid, formic acid, hydrochloric acid, nitric acid, citric acid, salicylic acid, tartaric acid, starch are all for chemical use; ammonium chloride, ammonium nitrate, ammonium sulfate Ammonium oxalate is an industrial product.
5. Pseudo boehmite (heat loss 36.2%), kaolin (heat loss 16.4%), halloysite (heat loss 21.4%), montmorillonite (heat loss 15.8%), perlite (heat loss 17.6%) are solid Aluminum sol contains 23.0% by weight aluminum oxide; silicon sol contains 24.5% by weight silica, both of which are industrially acceptable.
6). REY, REHY, USY, and REUSY molecular sieve are all acceptable industrial products, manufactured by Lanzhou Petrochemical Co., Ltd .; β- zeolites are industrially acceptable products, manufactured by Fushunishi Chemical; H-ZSM-5 is industrially acceptable products, Made by Shanghai Fudan University.
水浴加熱付の反応槽に、水4.620リットル、カオリン1024g、擬ベーマイト971g及び塩酸90.8mlを添加して均一に混合し、1時間攪拌した後、変性モレキュラーシーブB-1 338g、βゼオライト129g、REHY 806gを順に添加し、均一に混合された後アルミニウムゾル1304gを徐々に加えゲル化し、噴霧成形を経て、得られた微小球を400℃で1.0時間焼成させた。焼成された微小球2kgを取り、脱イオン水20kgを入れて35℃で40分間洗浄し、濾過乾燥して本発明に調製される分解触媒が得られ、Bと表記する。 In a reaction bath with water bath heating, 4.620 liters of water, 1024 g of kaolin, 971 g of pseudoboehmite and 90.8 ml of hydrochloric acid were added and mixed uniformly. After stirring for 1 hour, 338 g of modified molecular sieve B-1 129 g of β zeolite, REHY 806 g was added in order, and after mixing uniformly, 1304 g of aluminum sol was gradually added to gel. After spray molding, the resulting microspheres were fired at 400 ° C. for 1.0 hour. Take 2 kg of calcined microspheres, add 20 kg of deionized water, wash at 35 ° C. for 40 minutes, filter and dry to obtain the cracking catalyst prepared in the present invention, which is denoted as B.
Claims (21)
超安定希土類Y型モレキュラーシーブは、希土類交換、分散予備交換を含む調製過程により得られるものであり、酸化希土類を0.5〜25重量%含み、酸化ナトリウムが1.2重量%以下、結晶化度が40〜75%、格子定数が2.449nm〜2.472nmであり、
希土類交換と分散予備交換は順次に限定されず連続して行われ、その間に焼成過程がなく、
分散予備交換は、モレキュラーシーブスラリーの濃度を固形分として80〜400g/Lに調整して、分散剤を0.2重量%〜7重量%加えて分散予備交換を行うものであり、交換温度が0〜100℃、交換時間が0.1〜1.5時間であり、
分散予備交換における上記の分散剤は、セスバニア粉、ホウ酸、尿素、エタノール、ポリアクリルアミド、酢酸、シュウ酸、アジピン酸、ギ酸、塩酸、硝酸、クエン酸、サリチル酸、酒石酸、安息香酸、デンプンから選ばれる1種又は1種以上のものであり、
希土類交換、分散予備交換においてアンモニウム塩が使用されないことを特徴とする重質油接触分解触媒。 In the composition of the catalyst, 2 to 50% by weight of ultra-stable rare earth Y-type molecular sieve, 0.5 to 30% by weight of one or more other molecular sieves, 0.5 to 70% by weight of clay, 1.0% of high-temperature inorganic oxide A heavy oil catalytic cracking catalyst comprising ~ 65 wt% and rare earth oxide 0.01 to 12.5 wt%,
The ultra-stable rare earth Y-type molecular sieve is obtained by a preparation process including rare earth exchange and dispersion pre-exchange, containing 0.5 to 25% by weight of rare earth oxide, 1.2% by weight or less of sodium oxide, and crystallinity of 40 to 40%. 75%, lattice constant is 2.449nm ~ 2.472nm,
Rare earth exchange and dispersion pre-exchange are not limited sequentially but are performed continuously, and there is no firing process between them,
In the dispersion pre-exchange, the concentration of the molecular sieve slurry is adjusted to 80 to 400 g / L as the solid content, and the dispersion pre-exchange is performed by adding 0.2 to 7 wt% of the dispersant, and the exchange temperature is 0 to 100 ° C, replacement time is 0.1-1.5 hours,
The above dispersant in the dispersion pre-exchange is selected from sesbania powder, boric acid, urea, ethanol, polyacrylamide, acetic acid, oxalic acid, adipic acid, formic acid, hydrochloric acid, nitric acid, citric acid, salicylic acid, tartaric acid, benzoic acid, starch One or more types
A heavy oil catalytic cracking catalyst characterized in that no ammonium salt is used in rare earth exchange or dispersion pre-exchange.
(1)NaYモレキュラーシーブを原料として、モレキュラーシーブスラリーが順次に限定されなく希土類交換、分散予備交換を経て、モレキュラーシーブスラリーをさらに濾過、水洗及び1回目焼成して、「1交換1焼成」希土類ナトリウムYモレキュラーシーブが得られ、「1交換1焼成」希土類ナトリウムYモレキュラーシーブをアンモニウム塩交換によるナトリウム低減し、2回目焼成して、超安定希土類Y型モレキュラーシーブが得られる超安定希土類Y型モレキュラーシーブの調製工程と、
(2)上記の超安定希土類Y型モレキュラーシーブと、クレー、耐高温無機酸化物の前駆体を混合均質化し、噴霧成形、焼成及び水洗して、触媒完成品が得られる重質油触媒の調製工程と、
を含むことを特徴とする請求項1に記載の触媒の製造方法。 During the catalyst production process,
(1) The molecular sieve slurry is not limited to the raw material, and the molecular sieve slurry is subjected to rare earth exchange and dispersion pre-exchange, and the molecular sieve slurry is further filtered, washed with water, and fired for the first time. Ultra-stable rare earth Y molecular sieves can be obtained by obtaining sodium Y molecular sieves, and reducing sodium by ammonium salt exchange in the “one-exchange-one-fired” rare earth sodium Y molecular sieves and firing the second time to obtain ultra-stable rare-earth Y-type molecular sieves. The sheave preparation process;
(2) Preparation of a heavy oil catalyst that can be obtained by mixing and homogenizing the above ultrastable rare earth Y-type molecular sieve with clay and high-temperature resistant inorganic oxide precursor, followed by spray molding, firing and washing with water. Process,
2. The method for producing a catalyst according to claim 1, comprising:
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CN201110419922.2A CN103157507B (en) | 2011-12-15 | 2011-12-15 | Heavy oil catalytic cracking catalyst and preparation method thereof |
PCT/CN2012/000508 WO2013086767A1 (en) | 2011-12-15 | 2012-04-13 | Heavy oil catalytic cracking catalyst and preparation method therefor |
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